Submerged self-suction rotating packed bed and application thereof

By designing a submerged self-priming rotary packed bed and combining the characteristics of centrifugal pumps and rotary packed beds, the problem of insufficient mixing in liquid-liquid heterogeneous reactions is solved, achieving uniform dispersion and self-priming capability of liquid materials, improving reaction selectivity and product yield, and making it suitable for various reaction and extraction equipment.

CN116550268BActive Publication Date: 2026-04-14BEIJING UNIV OF CHEM TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-16
Publication Date
2026-04-14

AI Technical Summary

Technical Problem

Existing rotating packed beds suffer from insufficient mixing and mass transfer resistance in liquid-liquid heterogeneous reactions, and traditional reactors cannot effectively improve reaction selectivity and product yield.

Method used

A submerged self-priming rotary packed bed is designed, combining the characteristics of a centrifugal pump and a rotary packed bed. Through a composite packing impeller and stator structure, it achieves uniform dispersion and self-priming capability of liquid materials, and is used as a premixing unit in conjunction with the main reactor.

Benefits of technology

It achieves optimal mixing of liquid materials before they enter the main reactor, improving reaction selectivity and product yield. It is suitable for various reaction and extraction equipment, especially for liquid-liquid homogeneous and heterogeneous systems.

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Abstract

The application discloses an immersed self-suction type rotating packed bed, which comprises a motor, a shell, a liquid inlet, a rotor assembly, a stator and a liquid outlet; the rotor assembly comprises a rotor, a composite filler impeller, a first rotating shaft and a second rotating shaft; the rotor is fixedly connected with the output shaft of the motor through the first rotating shaft; the second rotating shaft is coaxial with the first rotating shaft and is arranged on the opposite side of the first rotating shaft, and the top end of the second rotating shaft is rollingly sleeved with the shell; the second rotating shaft is a hollow channel structure, and the end of the liquid inlet is connected with the hollow channel of the second rotating shaft; the composite filler impeller comprises annular fillers, inner vanes and outer vanes; the inner vanes are fixedly arranged on the inner side of the annular fillers, and the outer vanes are fixedly arranged on the outer side of the annular fillers. The rotating packed bed has the mixing characteristics of the rotating packed bed and the conveying characteristics of the centrifugal pump, and as a pre-reactor, the material can reach the best mixing state before entering the main reactor.
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Description

Technical Field

[0001] This invention relates to the field of rotary filling bed technology. More specifically, it relates to an immersion self-priming rotary filling bed and its application. Background Technology

[0002] Currently, rotating packed beds are one of the representative equipment in process intensification technology. Through high-speed rotating packing, the rotating packed bed cuts the liquid phase into fine liquid micro-elements, greatly increasing the mass transfer surface area and surface renewal rate. In liquid-liquid heterogeneous reactions, the reaction process usually occurs at the interface between the two phases, where interphase mass transfer resistance exists. Therefore, the mass transfer surface area and mixing degree between the two phases are key parameters in liquid-liquid heterogeneous reactions. Good mass transfer performance of the reactor can significantly improve the selectivity of the reaction and the yield of the product. Since traditional reactors, such as tubular reactors, suffer from insufficient mixing, this invention develops a self-priming, submerged fluid-driven rotating packed bed that also serves as a premixing unit for the main reactor. This allows the two-phase fluids to fully contact and mix before entering the main reactor, achieving a streamlined reaction process and high efficiency. It has broad application prospects in organic chemical engineering, polymer chemical engineering, and other fields. Summary of the Invention

[0003] The first technical problem to be solved by this invention is to provide a submerged self-priming rotary packed bed. This submerged self-priming rotary packed bed combines the mixing characteristics of a rotary packed bed with the conveying characteristics of a centrifugal pump, serving as a pre-reactor to ensure that the material reaches an optimal mixing state before entering the main reactor.

[0004] The second technical problem to be solved by the present invention is to provide an application of an immersion self-priming rotary filling bed.

[0005] To solve the first technical problem mentioned above, the invention adopts the following technical solution:

[0006] A submersible self-priming rotary filled bed includes: a motor, a housing, a liquid inlet, a rotor assembly, a stator, and a liquid outlet;

[0007] The rotor assembly includes a rotor, a composite packing impeller, a first rotating shaft, and a second rotating shaft;

[0008] The rotor is fixedly connected to the output shaft of the motor via a first rotating shaft;

[0009] The second rotating shaft and the first rotating shaft are aligned at their centers and are located on opposite sides. The top end of the second rotating shaft is rolled into the housing.

[0010] The second rotating shaft has a hollow channel structure, and the end of the liquid inlet leads to the hollow channel of the second rotating shaft;

[0011] The composite packing impeller includes annular packing, inner impeller blades, and outer impeller blades; the inner impeller blades are fixed on the inner side of the annular packing and on the outer side of the annular packing.

[0012] Preferably, the annular packing comprises multiple layers, with gaps between each layer of annular packing; one end of the stator is fixed to the inner wall of the housing, and the other end extends into the gaps between the annular packing.

[0013] Preferably, the liquid inlet includes a main liquid inlet and a secondary liquid inlet; the secondary liquid inlet is connected to the secondary liquid inlet channel, and the main liquid inlet is connected to the main liquid inlet channel.

[0014] More preferably, the secondary liquid inlet channel extends into the main liquid inlet channel.

[0015] More preferably, the secondary liquid inlet channel surrounds the main liquid inlet channel; the secondary liquid inlet is located on the side wall of the secondary liquid inlet channel; the main liquid inlet channel and the secondary liquid inlet channel are connected by a through hole provided on the side wall of the main liquid inlet channel.

[0016] More preferably, the main liquid inlet channel adopts a Venturi tube structure.

[0017] Preferably, the inner blades and outer blades of the impeller are straight blades or curved blades.

[0018] Preferably, the number of inner and outer blades of the impeller is 6-12, and they are evenly arranged on the annular packing.

[0019] Preferably, the annular packing is a metal wire mesh packing, a 3D printed packing, or a porous plate packing.

[0020] To solve the second technical problem mentioned above, the invention adopts the following technical solution:

[0021] An application of a submersible self-priming rotary packed bed in a liquid-liquid homogeneous and heterogeneous mixing system;

[0022] Preferably, the two liquids enter from the liquid inlet, are dispersed and fully mixed by the rotor, and the mixture flows out from the liquid outlet.

[0023] Preferably, the submerged self-priming rotary packed bed is used in conjunction with a batch reactor;

[0024] Preferably, the submerged self-priming rotary packed bed is used in conjunction with a tubular reactor;

[0025] Preferably, the submerged self-priming rotary packed bed is used in conjunction with a mixing and clarification tank.

[0026] Any range described in this invention includes the endpoint, any value between the endpoints, and any subrange consisting of the endpoint or any value between the endpoints.

[0027] Unless otherwise specified, all raw materials used in this invention can be obtained commercially, and the equipment used in this invention can be conventional equipment in the relevant field or refer to existing technology in the relevant field.

[0028] 1) The submerged self-priming rotary packed bed designed in this invention achieves equipment integration, combines the characteristics of centrifugal pumps and rotary packed beds, and has both mixing and pumping characteristics. It utilizes a rotor structure that combines impeller and packing, supplemented by stator and structure, to achieve uniform dispersion of liquid materials.

[0029] 2) The submerged self-priming rotating packed bed designed in this invention has a wide range of applications and can be combined with various reaction equipment and extraction equipment. As a pre-processing part of the overall equipment, it meets the mixing state required when the material enters the main reactor. It is especially suitable for liquid-liquid homogeneous and heterogeneous systems under different working conditions.

[0030] 3) The submerged self-priming rotary packed bed rotor component designed in this invention adopts a submerged form, which can provide self-priming capability and enhance mass transfer through the rotation of the composite packing impeller. At the same time, the flow rate and dispersion capability can be controlled by adjusting the size and speed of the rotor component. Attached Figure Description

[0031] The specific embodiments of the present invention will be further described in detail below with reference to the accompanying drawings.

[0032] Figure 1 This is a schematic diagram of one embodiment of the submersible self-priming rotary filling bed of the present invention;

[0033] Figure 2 This is a schematic diagram of the rotor component of the submerged self-priming rotary filling bed of the present invention;

[0034] Figure 3 This is a schematic diagram of another embodiment (statorless structure) of the immersion self-priming rotary filling bed of the present invention;

[0035] Figure 4 This is a schematic diagram of another embodiment of the submersible self-priming rotary filling bed of the present invention;

[0036] Figure 5 This is a schematic diagram of the structure of the sleeve-type liquid inlet submerged self-priming rotary packed bed of the present invention;

[0037] Figure 6 This is a schematic diagram of the Venturi tube type liquid inlet submerged self-priming rotary packed bed structure of the present invention;

[0038] Figure 7This is a process flow diagram of the combined use of the submerged self-priming rotary packed bed and the batch reactor of the present invention;

[0039] Figure 8 This is a process flow diagram of the combined use of the submerged self-priming rotary packed bed and tubular reactor of the present invention;

[0040] Figure 9 This is a process flow diagram of the combined use of the submerged self-priming rotary packed bed and the mixing and clarification tank of the present invention. Detailed Implementation

[0041] To more clearly illustrate the present invention, the following description, in conjunction with preferred embodiments and accompanying drawings, further explains the invention. Similar components in the drawings are indicated by the same reference numerals. Those skilled in the art should understand that the specific description below is illustrative rather than restrictive and should not be construed as limiting the scope of protection of the present invention.

[0042] Various cross-sectional views of embodiments of the present invention are shown in the accompanying drawings. These drawings are not to scale, and some details have been enlarged for clarity, and some details may have been omitted. The shapes of the various regions and layers shown in the drawings, as well as their relative sizes and positional relationships, are merely exemplary and may deviate from reality due to manufacturing tolerances or technical limitations. Furthermore, those skilled in the art can design regions / layers with different shapes, sizes, and relative positions as needed.

[0043] Currently, rotating packed beds are one of the representative pieces of equipment in process intensification technology. Through high-speed rotating packing material, the rotating packed bed cuts the liquid phase into tiny liquid micro-elements, greatly increasing the mass transfer surface area and surface renewal rate. In liquid-liquid heterogeneous reactions, the reaction process usually occurs at the interface between the two phases, where interphase mass transfer resistance exists. Therefore, the mass transfer surface area and the degree of mixing between the two phases are key parameters in liquid-liquid heterogeneous reactions. Good mass transfer performance of the reactor can significantly improve the selectivity of the reaction and the yield of the product.

[0044] Based on this, such as Figure 3 As shown, as one aspect of the present invention, the present invention provides an immersion self-priming rotary filling bed, including a motor 6, a housing 4, a liquid inlet 1, a rotor assembly 3 and a liquid outlet 5;

[0045] The rotor assembly 3 includes a rotor 31, a composite packing impeller 32, a first rotating shaft 33, and a second rotating shaft 34.

[0046] The rotor 31 is fixedly connected to the output shaft 61 of the motor 6 via the first rotating shaft 33;

[0047] The second rotating shaft 34 and the first rotating shaft 33 are aligned at their centers and are positioned on opposite sides (i.e., the first rotating shaft 33 extends to the right in the figure, and the second rotating shaft 34 extends to the left). The top end of the second rotating shaft 34 is rolled into the housing 4. It can be understood that the first rotating shaft 33 and the second rotating shaft 34 not only undertake the task of rotation, but also serve as the load-bearing rotor assembly 3 of the central shaft.

[0048] The second rotating shaft 34 has a hollow channel structure, and the end of the liquid inlet leads to the hollow channel of the second rotating shaft;

[0049] See Figure 2 As shown, the composite packing impeller 32 includes annular packing 321, inner impeller blades 322, and outer impeller blades 323. The inner impeller blades 322 are fixed to the inner side of the annular packing 321, and the outer impeller blades 323 are fixed to the outer side of the annular packing 321. As those skilled in the art will understand, when the composite packing impeller 32 rotates, the liquid passes through the inner impeller blades 322 and the annular packing 321 and is thrown to the outer edge of the outer impeller blades 323. A negative pressure state is formed at the inlet of the inner impeller blades 322, and the liquid is continuously drawn into the impeller at the liquid inlet to achieve a self-priming effect.

[0050] The liquid inlet 1 includes a main liquid inlet 11 and a secondary liquid inlet 12; the secondary liquid inlet 12 is connected to the secondary liquid inlet channel 121, and the main liquid inlet 11 is connected to the main liquid inlet channel 111.

[0051] According to certain embodiments of the present invention, such as Figure 1 or Figure 2 As shown, the annular packing 321 includes two layers, and a gap 324 is provided between the two layers of annular packing; at this time, the rotating packing bed is also provided with a stator 2, one end of which is fixed on the inner wall of the shell 4, and the other end extends into the gap 324 between the multiple layers of annular packing 321.

[0052] In some embodiments, see Figure 4 As shown, the secondary liquid inlet channel 121 extends into the main liquid inlet channel 111.

[0053] In some embodiments, see Figure 5 and Figure 6 As shown, the secondary liquid inlet channel 121 surrounds the outside of the main liquid inlet channel 111; the secondary liquid inlet 12 is located on the side wall of the secondary liquid inlet channel 121; the main liquid inlet channel 111 and the secondary liquid inlet channel 121 are connected by a through hole 112 provided on the side wall of the main liquid inlet channel 111.

[0054] In some embodiments, see Figure 6As shown, the main liquid inlet channel 111 adopts a Venturi tube structure.

[0055] In some embodiments, the inner blade 322 and the outer blade 323 of the impeller are straight blades or curved blades.

[0056] In some embodiments, the number of inner impeller blades 322 and outer impeller blades 323 is 6-12, which are evenly arranged on the annular packing 321.

[0057] In some embodiments, the annular packing 321 is a metal wire mesh packing, a 3D printed packing, or a porous plate packing.

[0058] As another aspect of the present invention, the present invention provides an application of an immersion self-priming rotary filling bed;

[0059] In some embodiments, the submerged self-priming rotary packed bed is applied to a liquid-liquid homogeneous and heterogeneous mixing system; preferably, the two liquids enter from the liquid inlet, are dispersed and fully mixed by the rotor, and the mixture flows out from the liquid outlet.

[0060] In some embodiments, the submerged self-priming rotating packed bed is used in conjunction with a batch reactor, which can be used for some liquid-liquid heterogeneous reaction systems with long reaction times and easy aggregation and stratification. The reactants are fully dispersed in the submerged self-priming rotating packed bed and transported to the batch reactor. Under the stirring action of the batch reactor, aggregation can be prevented and the reaction time can be extended.

[0061] In some embodiments, the submerged self-priming rotating packed bed is used in conjunction with a tubular reactor. This can be used in some liquid-liquid homogeneous or heterogeneous reaction systems with intense heat absorption and release. The reactants are transported to the tubular reactor after a very short residence time in the submerged self-priming rotating packed bed. In the tubular reactor, the heat inside the reaction system can be transferred in a timely and efficient manner, effectively avoiding the problem of excessively high local hot spots in the reaction system that affect product quality.

[0062] In some embodiments, the submerged self-priming rotating packed bed is used in conjunction with a mixing and clarification tank for liquid-liquid heterogeneous extraction systems. The solution is first intensified in the submerged self-priming rotating packed bed for mixing and dispersion, and then enters the mixing and clarification tank for further extraction, which greatly shortens the extraction time and improves the extraction efficiency.

[0063] Example 1

[0064] See Figure 1 As shown, the silicone oil-water system dispersion experiment was conducted using the submerged self-priming rotating packed bed of this invention:

[0065] Tween 80 at a mass fraction of 2% was added to kerosene as a surfactant. The impeller of the submerged self-priming rotary packed bed rotated to draw water from the water tank into the rotary packed bed through the secondary liquid inlet 11. The kerosene with surfactant was introduced through the secondary liquid inlet 12. After the two phases were fully mixed, they flowed out through the outlet. The particle size distribution of the silicone oil at the outlet was measured by a laser particle size analyzer. The average particle size of the obtained silicone oil was in the range of 50 to 600 nm.

[0066] Example 2

[0067] See Figure 3 As shown, Example 1 is repeated, except that:

[0068] The immersed self-priming rotary packed bed has no stator structure, and the average particle size of the resulting silicone oil is 100-1000 nm.

[0069] Example 3

[0070] See Figure 7 As shown, the biodiesel production reaction is carried out by combining the submerged self-priming rotating packed bed of the present invention with a batch reactor:

[0071] The feedstock is pure corn oil, methanol is used to react with the feedstock, and potassium hydroxide (KOH) is used as a catalyst in the transesterification reaction.

[0072] This transesterification reaction involves three main kinetic processes:

[0073] The first is the initial mass transfer stage, which is the mixing stage of oil and methanol, during which methanol and corn oil are not yet immiscible.

[0074] The second stage is the chemical kinetic control stage, in which fatty acid methyl esters begin to form and rapidly enhance the reaction by increasing the contact area between the two liquids; in this second stage, the effect of stirring is significantly reduced because the kinetics increase spontaneously through the reaction between molecules in the two phases.

[0075] The third stage is the equilibrium stage, where the reactants decrease and the product formation cannot be enhanced by further stirring.

[0076] The experimental procedure was as follows: Methanol (A) and feedstock oil (B) were drawn into a submerged self-priming rotating packed bed through a liquid storage tank via a secondary liquid inlet and a main liquid inlet, respectively, at a molar ratio of 6:1. The catalyst was a 1.6% KOH solution (C) which was introduced through the secondary liquid inlet. The yield of fatty acid methyl esters of each method was compared within 30 minutes of reaction between using a submerged self-priming rotating packed bed in combination with a stirred tank and using a stirred tank alone.

[0077] Data shows that when the submerged self-priming rotary packed bed is used in conjunction with the stirred tank, the yield of fatty acid methyl esters at the liquid outlet reaches its maximum value and remains stable 1 minute after startup, while the yield of the stirred tank reaches its maximum value after 10 to 15 minutes and then slowly stabilizes.

[0078] The results showed that the fatty acid methyl ester yield of the batch reactor was relatively low in the first stage of the reaction. This was because the batch reactor could not provide sufficient mixing strength to mix the immiscible methanol and oil. However, when combined with a submerged self-priming rotating packed bed, the fine methanol droplets could be uniformly dispersed in the oil, which significantly increased the surface area of ​​the interface between the oil and methanol.

[0079] Example 4

[0080] See Figure 8 As shown, the nitration reaction is carried out by using the submerged self-priming rotating packed bed of the present invention in combination with a tubular reactor:

[0081] The reaction feedstocks are a benzene / nitrobenzene mixture (A) and a nitric acid-sulfuric acid mixture (B), stored separately in liquid tanks. The volume ratio of benzene to nitrobenzene is 1:4, and the volume ratio of nitric acid to sulfuric acid is 1:7. The benzene / nitrobenzene mixture enters through the main liquid inlet, while the nitric acid-sulfuric acid mixture enters through the secondary liquid inlet. The submerged self-aspirating rotating packed bed operates at 600 rpm. After the reaction stabilizes, the benzene content in the organic phase after the reaction is determined by gas chromatography, and the benzene conversion rate is calculated to be >99.5%. Besides nitration, the combined use of a submerged self-aspirating rotating packed bed reactor and a tubular reactor is also suitable for sulfonation, polymerization, rearrangement, and diazotization reactions.

[0082] Example 5

[0083] See Figure 9 As shown, the submerged self-priming rotating packed bed of this invention is used in conjunction with a tubular reactor for liquid-liquid heterogeneous extraction reactions:

[0084] The extraction system consisted of a kerosene solution of 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester in the light phase, with a volume percentage of 30%. The heavy phase was an aqueous sulfuric acid solution with pH 3.5 containing cobalt ions, at a concentration of 0.8 g / L. A sample of the heavy phase was collected from the outlet and sent for analysis; the cobalt extraction rate was 96%.

[0085] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the implementation of the present invention. Those skilled in the art can make other variations or modifications based on the above description. It is impossible to exhaustively list all embodiments here. All obvious variations or modifications derived from the technical solutions of the present invention are still within the protection scope of the present invention.

Claims

1. A submersible self-priming rotary packed bed, comprising a motor, a housing, a liquid inlet, a rotor assembly, a stator, and a liquid outlet; characterized in that: The rotor assembly includes a rotor, a composite packing impeller, a first rotating shaft, and a second rotating shaft; The rotor is fixedly connected to the output shaft of the motor via a first rotating shaft; The second rotating shaft and the first rotating shaft are aligned at their centers and are located on opposite sides. The top end of the second rotating shaft is rolled into the housing. The second rotating shaft has a hollow channel structure, and the end of the liquid inlet leads to the hollow channel of the second rotating shaft; The composite packing impeller includes annular packing, inner impeller blades, and outer impeller blades; the inner impeller blades are fixed on the inner side of the annular packing and on the outer side of the annular packing.

2. The submersible self-priming rotary filling bed according to claim 1, characterized in that: The annular packing comprises multiple layers, with gaps between each layer of annular packing; one end of the stator is fixed to the inner wall of the housing, and the other end extends into the gaps between the annular packing.

3. The submersible self-priming rotary filling bed according to claim 1, characterized in that: The liquid inlet includes a main liquid inlet and a secondary liquid inlet; the secondary liquid inlet is connected to the secondary liquid inlet channel, and the main liquid inlet is connected to the main liquid inlet channel.

4. The submersible self-priming rotary filling bed according to claim 3, characterized in that: The secondary liquid inlet channel extends into the main liquid inlet channel.

5. The submersible self-priming rotary filling bed according to claim 4, characterized in that: The secondary liquid inlet channel surrounds the main liquid inlet channel; the secondary liquid inlet is located on the side wall of the secondary liquid inlet channel; the main liquid inlet channel and the secondary liquid inlet channel are connected by a through hole provided on the side wall of the main liquid inlet channel.

6. The submersible self-priming rotary filling bed according to claim 3, characterized in that: The main liquid inlet channel adopts a Venturi tube structure.

7. The submersible self-priming rotary filling bed according to claim 3, characterized in that: The secondary liquid inlet is provided in multiple locations.

8. The submersible self-priming rotary filling bed according to claim 1, characterized in that: The inner and outer blades of the impeller are straight or curved blades. The number of inner and outer blades of the impeller is 6-12, and they are evenly arranged on the annular packing. The annular packing is a metal wire mesh packing, a 3D printed packing, or a porous plate packing.

9. The application of the submersible self-priming rotary filling bed as described in any one of claims 1-8, characterized in that: The submerged self-priming rotary packed bed is applied to liquid-liquid homogeneous and heterogeneous mixing systems; the two liquids enter from the liquid inlet respectively, are fully mixed by the rotor dispersion, and the mixture flows out from the liquid outlet.

10. The application according to claim 9, characterized in that: The submerged self-priming rotary packed bed is used in conjunction with a batch reactor.

11. The application according to claim 9, characterized in that: The submerged self-priming rotating packed bed is used in conjunction with a tubular reactor.

12. The application according to claim 9, characterized in that: The submerged self-priming rotary packed bed is used in conjunction with a mixing and clarification tank.